CN113853400A - Aqueous dispersion composition - Google Patents
Aqueous dispersion composition Download PDFInfo
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- CN113853400A CN113853400A CN202080036986.1A CN202080036986A CN113853400A CN 113853400 A CN113853400 A CN 113853400A CN 202080036986 A CN202080036986 A CN 202080036986A CN 113853400 A CN113853400 A CN 113853400A
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- Prior art keywords
- extruder
- dispersion
- fed
- feeding
- vinyl acetate
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- 239000006185 dispersion Substances 0.000 title claims abstract description 121
- 239000000203 mixture Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229920001577 copolymer Polymers 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- 238000010924 continuous production Methods 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 47
- 239000002245 particle Substances 0.000 claims description 38
- 239000007787 solid Substances 0.000 claims description 37
- 238000000576 coating method Methods 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 25
- 238000007792 addition Methods 0.000 claims description 19
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 9
- 235000013305 food Nutrition 0.000 claims description 9
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 9
- 238000004806 packaging method and process Methods 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 239000000758 substrate Substances 0.000 description 27
- 150000001875 compounds Chemical class 0.000 description 25
- 210000003995 blood forming stem cell Anatomy 0.000 description 24
- 238000010923 batch production Methods 0.000 description 19
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- 239000003795 chemical substances by application Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 230000003472 neutralizing effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- -1 alkyl carboxylic acid Chemical class 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 239000013065 commercial product Substances 0.000 description 5
- 238000004945 emulsification Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- 238000004383 yellowing Methods 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 239000012768 molten material Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000003442 weekly effect Effects 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 239000004775 Tyvek Substances 0.000 description 1
- 229920000690 Tyvek Polymers 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 238000007718 adhesive strength test Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000007754 air knife coating Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical group C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 238000009466 skin packaging Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000010947 wet-dispersion method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D131/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Coating compositions based on derivatives of such polymers
- C09D131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09D131/04—Homopolymers or copolymers of vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J131/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
- C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09J131/04—Homopolymers or copolymers of vinyl acetate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
- H01L21/31116—Etching inorganic layers by chemical means by dry-etching
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2331/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
- C08J2331/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
- C08J2331/04—Homopolymers or copolymers of vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Paints Or Removers (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Drying Of Semiconductors (AREA)
Abstract
A method for preparing an aqueous dispersion composition made using an extruder-based continuous process comprising the steps of: (A) providing an extruder; (B) feeding into the extruder a mixture of: (i) at least one vinyl acetate copolymer; (ii) at least one compatibilizer; and a dispersant; (C) feeding a first aqueous additive to the mixture of step (B) in the extruder to provide a continuous dispersion of polymer; (D) feeding at least one base to the mixture of step (C) in the extruder to neutralize any available acid present in the mixture of step (C); and (E) feeding a second water addition to the mixture of step (D) in the extruder to effect a phase inversion to form an aqueous continuous dispersion.
Description
Technical Field
The present invention relates to an aqueous dispersion composition for use as a Heat Seal Coating (HSC); more particularly, the present invention relates to an aqueous dispersion composition for use as HSC produced by an extruder-based continuous phase inversion process.
Background
In the food and industrial packaging industry, adhesive compositions are commonly used to heat seal polymer packages at low temperatures (e.g., less than [ < ]150 degrees Celsius [ ° C ]); at low temperatures, the adhesive composition should: (1) stable, (2) has reasonable particle size and particle size distribution, (3) viscosity and rheological properties allow the composition to be easily applied to a substrate and can be coated on a substrate to provide a uniform heat seal coating; (4) is environment-friendly, and (5) meets the requirements of food contact regulations, so that the food packaging bag is suitable for food packaging.
Heretofore, low temperature heat seal compositions for use as emulsion adhesive products have been prepared using various emulsification processes under various process conditions (e.g., at elevated temperature and pressure), for example as disclosed in CN108084370A, CN108148215A, and CN 108102472A. In addition, extruder-based continuous direct dispersion processes have also been used to prepare waterborne heat seal products based on ethylene-vinyl acetate copolymers (EVA copolymers) in which a polymer melt blend is contacted with an aqueous stream comprising a neutralizing agent, water and a surfactant in an emulsification zone of an extruder to form a dispersion. However, the above direct emulsification processes suffer from one or more problems, such as the relatively broad particle size distribution of the emulsions produced by the process, which can lead to potential coating appearance problems, such as yellowing, potentially reduced shelf-life stability, non-uniformity of particle composition from particle to particle, and the like. In view of the above-presented problems of the prior art emulsions and processes, it would be desirable to provide a dispersion composition that can be used as a heat seal coating that does not suffer from the above problems.
Disclosure of Invention
The present invention relates to a novel aqueous vinyl acetate copolymer dispersion composition for use as HSCs. According to a preferred embodiment of the present invention, the vinyl acetate copolymer may comprise, for example, an Ethylene Vinyl Acetate (EVA) copolymer dispersion composition. In another preferred embodiment, the dispersion composition may comprise the following components: (a) at least one vinyl acetate copolymer; (b) at least one compatibilizer; (c) at least one alkyl carboxylic acid as a dispersant after neutralization; (d) a first water addition to provide a continuous dispersion of polymer; (e) at least one base added for neutralization of available acid and separation of water additives that continuously produce a continuous system of polymers; and (f) a second water addition to effect phase conversion to a water continuous dispersion.
In another embodiment, the invention includes a method of making an aqueous vinyl acetate copolymer dispersion composition for use as a HSC, wherein the method comprises producing the dispersion using an extruder-based continuous phase inversion process. The process is advantageous because it is capable of producing dispersions with smaller particle size and narrower particle size distribution and lower amounts of surfactant (e.g., <1.5 weight% [ wt% ]) than direct emulsification processes using continuous extruders. The use of increased amounts (e.g., greater than [ > ]2 weight%) of surfactant can adversely affect the application properties of the resulting dispersion product, such as lower water resistance and lower durability due to surfactant surface migration.
In yet another embodiment, the present invention includes HSCs prepared from the above dispersion composition; and a substrate containing HSCs on at least a portion of a surface of the substrate.
In yet another embodiment, the present invention includes food and industrial packaging materials heat sealed with the above HSCs; and heat-sealable articles prepared from the above HSC compositions.
Detailed Description
"compatibilizer" herein means a resin having a viscosity at 170 ℃ of >1 pascal-second (Pa · s) and an acid number between 50 milligrams of potassium hydroxide (KOH) per gram of resin (mg KOH/g resin) and 200 milligrams KOH/g resin; and a melting point above 100 ℃.
By "dispersant" herein is meant a fatty acid, a soap produced in situ.
By "neutralizing agent" herein is meant a compound used to neutralize an acid (e.g., an alkyl carboxylic acid as described herein). Examples of neutralizing agents include, for example, KOH, ammonia, NaOH, amines, and mixtures thereof.
Water herein means Deionized (DI) water used to make the aqueous dispersion of the present invention.
In a broad embodiment, the dispersion composition of the present invention comprises: (a) at least one vinyl acetate copolymer, such as EVA; (b) at least one compatibilizer; (c) at least one dispersant; (d) a first water addition to provide a continuous dispersion of polymer; (e) at least one base added for neutralization of available acid and separation of water additives that continuously produce a continuous system of polymers; and (f) a second water addition to effect phase conversion to a water continuous dispersion.
The vinyl acetate copolymer compound used to prepare the dispersion composition of the present invention comprises, for example, one or more vinyl acetate copolymer compounds known in the art. For example, the copolymer compound comprises ethylene vinyl acetate copolymer (EVA); vinyl acetate ethylene copolymer (VAE); other vinyl acetate copolymers such as vinyl acetate acrylate copolymers and vinyl acetate-ethylene-styrene copolymers and the like; and mixtures thereof.
The amount of copolymer compound used to prepare the dispersion composition of the present invention is, for example, from 50 to 90 weight percent in one embodiment, from 80 to 90 weight percent in another embodiment, and from 85 to 90 weight percent in yet another embodiment, based on total solids content.
Some exemplary advantageous properties exhibited by vinyl acetate copolymer compounds may include better adhesion to polyethylene terephthalate (PET), foil, and other substrates.
In another embodiment, the copolymer is produced, for example, using an oxygen-containing monomer as one of the monomers (i.e., comonomer with vinyl acetate comonomer). For example, in addition to the olefin, e.g., ethylene, the comonomer is selected from one or more of the following compounds: vinyl acetate, acrylates, methacrylates, acrylic nitriles, and the like; and mixtures thereof.
The amount of comonomer compound when used with a vinyl acetate comonomer is, for example, from 5 to 70 weight percent in one embodiment, from 10 to 50 weight percent in another embodiment, from 15 to 40 weight percent in yet another embodiment, and from 15 to 30 weight percent in yet another embodiment.
The compatibilizer compound used to prepare the dispersion compositions of the present invention comprises, for example, one or more compatibilizer compounds known in the art. For example, in one embodiment, the compatibilizer compound comprises a rosin acid, a rosin ester, a terpene phenolic resin, a pure monomer resin, and a phenolic resin, or mixtures thereof.
Generally, the viscosity of the compatibilizer compound at 170 ℃ is >1Pa · s in one embodiment, from 1Pa · s to 20Pa · s in another embodiment, and from 5Pa · s to 8Pa · s in yet another embodiment. The viscosity of the compatibilizer is measured by any well known means, such as by using a conventional viscometer, such as Boehler fly Thermosel (Brookfield Thermosel).
Generally, the compatibilizer compound has the following acid number: in one embodiment from 10mg KOH/g resin to 250mg KOH/g resin, in another embodiment from 50mg KOH/g resin to 200mg KOH/g resin, in yet another embodiment from 100mg KOH/g resin to 200mg KOH/g resin, in yet another embodiment from 125mg KOH/g resin to 200mg KOH/g resin, and in even yet another embodiment from 140mg KOH/g resin to 180mg KOH/g resin. The acid number of the compatibilizer can be measured by any conventional titration method.
The melting point of the compatibilizer compound includes, for example, above 40 ℃ in one embodiment, from 50 ℃ to 200 ℃ in another embodiment, from 100 ℃ to 200 ℃ in yet another embodiment, and from 120 ℃ to 180 ℃ in yet another embodiment. The melting point of the compatibilizer can be measured by any well known means. For example, the melting point of the compatibilizer of the present invention is measured by a conventional Differential Scanning Calorimetry (DSC) method.
The amount of compatibilizer compound used to prepare the dispersion compositions of the present invention includes, for example, from 5 to 30 weight percent of the total solids content in one embodiment, from 9 to 20 weight percent in another embodiment, from 9 to 15 weight percent in yet another embodiment, and from 9 to 12 weight percent in yet another embodiment.
Some benefits of using compatibilizer compounds include, for example, the compatibilizer allows the EVA polymer to readily interact with the dispersant, and the compatibilizer allows the EVA polymer to readily interact with the substrate, which can enhance adhesive performance.
The dispersant or dispersant compound used to prepare the dispersion compositions of the present invention includes, for example, one or more dispersants known in the art. For example, in one embodiment, the dispersant comprises an alkyl carboxylic acid; oleic acid (fatty acid, soap generated in situ); a dimer acid; other alkyl carboxylic acids having from >12 to <20 carbon atoms per acid; and mixtures thereof.
The concentration of dispersant used to prepare the dispersion compositions of the present invention includes, for example, < 2% by weight of the solids of the formulation in one embodiment, in another embodiment < 1.5% by weight, in yet another embodiment < 1% by weight, in yet another embodiment from 0.66% to 1% by weight, and in even another embodiment from 0.66% to 0.75% by weight.
When the correct amount of dispersant is properly selected, some exemplary advantageous properties include (1) providing stability to the polymer particles in the dispersion, and (2) providing a balance of the surface tension and wetting ability of the dispersion to the substrate.
The method of making the dispersion composition of the present invention may comprise adding one or more water additives to the composition. For example, in one preferred embodiment, the first aqueous additive is added to the composition in an amount sufficient to form a continuous dispersion of the polymer.
For example, the amount of the first water addition is 3.5 wt% to 6 wt% in one embodiment, 3.5 wt% to 5 wt% in another embodiment, and 3.5 wt% to 4.5 wt% in yet another embodiment, based on total solids and water.
The dispersion composition of the present invention includes a base to neutralize the available acid in the composition and separate the water addition which continuously produces a continuous system of polymer. The base compound used to prepare the dispersion composition of the present invention includes, for example, one or more bases known in the art. For example, neutralizing agents or base compounds include aqueous potassium hydroxide (KOH), sodium hydroxide (NaOH), ammonia, and mixtures thereof. In a preferred embodiment, the base compound is, for example: in another embodiment from 10 to 90 wt.%, from 20 to 90 wt.%, and in yet another embodiment KOH having a concentration of from 40 to 50 wt.%.
The amount of base used to prepare the dispersion composition of the present invention is, for example: in one embodiment, the theoretical neutralization acid number of the components is 70 percent (%) to 130%, in another embodiment, 80% to 120%, in yet another embodiment, 90% to 110%, and in yet another embodiment, 90% to 100%.
Some exemplary advantageous properties exhibited by bases may include neutralization to stabilize the polymer particles.
As previously mentioned, the method of making the dispersion composition of the present invention comprises adding one or more water to the composition. In a preferred embodiment, a second water addition is added to the composition, for example in an amount sufficient to effect a phase transition into a water continuous dispersion.
For example, the amount of the second water addition is >3.5 wt% in one embodiment, 20 wt% to 90 wt% in another embodiment, 30 wt% to 70 wt% in yet another embodiment, and 40 wt% to 60 wt% in yet another embodiment, based on (1) total solids, (2) the first water addition, and (3) the second water addition.
The dispersion composition of the present invention may also include optional other additional compounds or additives; and the optional compound may be added to the composition in combination with one or more of components (a) - (f). Optional additives or agents useful in preparing the dispersion compositions of the present invention include, for example, one or more optional compounds known in the art for their use or function. For example, optional additives include, but are not limited to, defoamers, rheology modifiers, wetting agents, and mixtures thereof.
When used to prepare the dispersion compositions of the present invention, the amount of optional compound includes, for example, from 0 wt% to 5 wt% in one embodiment, from 0.001 wt% to 3 wt% in another embodiment, from 0.01 wt% to 2 wt% in yet another embodiment, and from 0.1 wt% to 1 wt% in yet another embodiment.
In a general embodiment, the process for preparing the dispersion composition of the present invention comprises the steps of intermixing (e.g., melt blending): (a) at least one vinyl acetate copolymer, such as EVA; (b) at least one compatibilizer; (c) at least one dispersant; (d) a first water addition to provide a continuous dispersion of polymer; (e) at least one base added for neutralization of available acid and separation of water additives that continuously produce a continuous system of polymers; and (f) a second water addition to effect phase conversion to a water continuous dispersion.
In general, the process equipment and ancillary equipment for forming a homogeneous molten blend suitable for use in the present invention may comprise any means; and any conditions commonly used for melt blending thermoplastic resins and known to those familiar with extruder-based processes. For example, it can be used in the present inventionThe device comprises a heat exchanger, a back pressure regulator, a melting pump and a gear pump; a kneader,
A mixer, a rotor-stator mixer, a single-screw extruder, a double-screw extruder, a multi-screw extruder and the like.
In addition, various schemes may be used to set up the process equipment. For example, in one embodiment, the first mixing device is used in combination with the second mixing device. For example, in some embodiments, the first mixing device is, for example, a kneader,
A mixer, a single screw extruder or a multi-screw extruder; and the second mixing device is, for example, an extruder, such as a twin screw extruder having a plurality of heating zones. For example, in other embodiments, the first mixing device is, e.g., an extruder, e.g., a twin screw extruder; and the second mixing device is a rotor-stator mixer.
In another embodiment, the aqueous dispersion composition of the present invention is produced using a single extruder (e.g., a twin screw extruder having multiple heating zones with ancillary equipment such as back pressure regulators, melt pumps or gear pumps). For example, in various embodiments, the extruder may have various zones, including, for example, (1) conveying, melting, and mixing zones, (2) emulsification zones, and (3) dilution zones; and the different zones may be operated at predetermined temperatures. In some embodiments, the conveying, melting, and mixing section portions of the extruder may have a barrel of length "L" and diameter "D" and the length to diameter ratio (L/D) used is: for example, in a preferred embodiment, no less than 12:1, such as 12:1 to 60: 1. In some preferred embodiments, the above-described extruder-based process used in the present invention is described in more detail in, for example, U.S. provisional patent application No. 62/579,354 filed by Escobar Marin et al, 2017, 10, 31.
In another embodiment, the aqueous dispersion composition is prepared, for example, using an extruder-based continuous process according to the following general method: the above components (a) - (f) of the composition of the present invention are fed into an extruder using, for example, a controlled rate feeder. As described above, any conventional extruder may be used in the present invention. In one embodiment, the extruder comprises a 25 millimeter (mm) diameter twin screw extruder, for example, having an L/D ratio as described above. In one embodiment, the feed rates (grams per minute (g/min)) of components (a) - (f) are, for example, 60g/min to 150 g/min. The components of the present invention are transferred through an extruder and melted to form a liquid molten material.
The extruder temperature profile may be stepped up to a predetermined temperature. For example, in one embodiment, the temperature ramp-up is 70 ℃ to 240 ℃, and in another embodiment 120 ℃ to 150 ℃. In one embodiment, water is then fed into the extruder at a predetermined rate (e.g., at a rate of 1.0g/min to 2.0 g/min). After the water is fed, the neutralizing agent is fed into the extruder using a second introduction point in the extruder in one embodiment at a predetermined rate (e.g., at a rate of 1.4g/min to 2.4 g/min). In one embodiment, the switching water is fed into the extruder via an inlet location of the extruder after the neutralizing agent; and water is fed into the extruder at a predetermined rate (e.g., at a rate of 1.0g/min to 8.0 g/min). In one embodiment, two separate pumps are also used to feed dilution water into the extruder at a predetermined rate (e.g., at a rate of 20g/min to 90 g/min) at one or both of the inlet locations (first and second inlet locations) of the extruder. The extruder temperature profile is re-cooled to a temperature below 100 c, for example, near the end of the extruder. At the extruder outlet, a back pressure regulator was used to adjust the pressure inside the extruder barrel to a pressure suitable to reduce steam formation. Generally, in one embodiment, the pressure inside the extruder barrel is, for example, 2 megapascals [ MPa ] to 4 MPa.
After the above procedural steps, the resulting aqueous dispersion product exits from the extruder. In a preferred embodiment, the aqueous dispersion is then filtered through a 200 micron (μm) filter. The resulting filtered aqueous dispersion has a solids content measured in weight percent (wt%); and the solid particles of the dispersion have a particle size in micronsVolume average particle size of the amount. For example, in one embodiment, the solids content of the dispersion is 30 wt% to 50 wt%; and in one embodiment, the particles in the dispersion have a particle size of 0.9 μm to 2.0 μm. In some embodiments, the granularity modulus value may also be recorded. Measuring the solids content of the aqueous dispersions using conventional instruments, e.g.
MB45 Infrared solid Analyzer (available from Ohaus Corporation); and also using conventional instrumentation (e.g. using
LS-230 particle size Analyzer (available from Beckman Coulter Corporation)) measures the particle size of the solid particles of the aqueous dispersion. In a preferred embodiment, the solid content and the average Particle Size (PS) of the solid particles of the dispersion are as described in table IV of the examples.
In one embodiment, the aqueous dispersion composition is, for example, a wax-free aqueous dispersion composition. In a preferred embodiment, the wax-free aqueous dispersion composition is manufactured, for example, using an extruder-based continuous process. The process steps include, for example, the following process steps:
(A) providing an extruder;
(B) feeding into the extruder a mixture of: (i) at least one vinyl acetate copolymer; (ii) at least one compatibilizer; and a dispersant;
(C) feeding a first aqueous additive to the mixture of step (B) in the extruder to provide a continuous dispersion of polymer;
(D) feeding at least one base to the mixture of step (C) in the extruder to neutralize any available acid present in the mixture of step (C); and
(E) feeding a second water addition to the mixture of step (D) in the extruder to effect a phase inversion to form an aqueous continuous dispersion.
In another embodiment, step (B) of the above method may be divided into two steps. For example, (i) at least one vinyl acetate copolymer and (ii) at least one compatibilizer are first mixed together to form a mixture, and then the mixture is fed into an extruder in the form of a stream; and feeding at least one dispersing agent to the extruder as a separate stream.
The dispersion compositions of the present invention prepared according to the methods described above have several beneficial properties, including, for example, smaller particle size and narrower particle distribution, and such properties advantageously result in, for example, good coating appearance; good coating uniformity; more preferably storage stability and preferably solids content.
For example, in one embodiment, the solids content of the dispersion of the present invention is from 20% solids to 80% solids; from 30% solids to 70% solids in another embodiment, and from 35% solids to 55% solids in yet another embodiment. The solids content of the dispersion can be measured, for example, by an aohaus MB45 infrared moisture analyzer (available from aohaus corporation) or by a hot oven. In a preferred embodiment, the solids content of the dispersion is measured by the above moisture analyzer.
For example, the viscosity characteristics of the dispersions of the present invention are in one embodiment from 10 millipascal-seconds (mpa.s) to 100 mpa.s; from 20mpa.s to 60mpa.s in another embodiment and from 30mpa.s to 50mpa.s in yet another embodiment. The viscosity properties of the dispersions were measured, for example, using Boehler fly DV-II + (from Boehler fly).
For example, the particle size of the particles in the dispersion of the present invention is in one embodiment 0.2 micrometers (μm) to 6 μm; in another embodiment 0.3 to 4 μm, and in yet another embodiment 0.4 to 2 μm. The particle size of the dispersion can be measured by any well-known particle size measuring instrument. In one embodiment, the particle size of the dispersion is measured, for example, using a beckmann coulter LS 13320 instrument.
In addition to the above characteristics, the performance of the dispersion composition was evaluated in terms of, for example, storage stability and tested by accelerated temperature aging under 45 ℃ and refrigerated conditions. For example, the storage stability of the dispersions of the invention is evaluated by aging in: (1) refrigerated (4 ℃) environment and (2) heated (45 ℃) oven, phase separation and viscosity of the dispersion were followed weekly. If the dispersion settles and separates into two layers; the viscosity is changed by over 100 percent; or becomes gel-like (i.e., gelation occurs), the dispersion is not stable to storage.
The overall stability of the dispersion can then be compared to a commercial product produced using a batch process. In one embodiment, the dispersion is rated in terms of, for example, "good" shelf stability or "worse" shelf stability compared to batch process products. For example, "good" shelf stability means a dispersion that performs as well as or better than a batch process commercial product; and "poorer shelf stability" means a poorer dispersion than the batch process commercial product.
As previously described, immediately after the dispersion composition of the present invention is prepared, the dispersion composition can be used for various applications as HSC. For example, in one embodiment, the HSC dispersion composition can be used to generate HSCs on a substrate such as a food packaging film, which can then be heat sealed.
The HSC dispersion composition can be applied to a substrate using various conventional coating methods, such as gravure coating, Meyer rod (Meyer rod) coating, curtain coating, air knife coating methods, flexographic methods, and lithographic methods.
The dispersion compositions of the present invention provide HSCs that can be advantageously used in various applications, such as for heat sealing food and industrial packaging. HSCs of the present invention also exhibit several beneficial properties, including for example: good coating appearance, high adhesive strength and high thermal tack, and is not yellowing.
For example, in one embodiment, the appearance of a coating formed from a HSC dispersion of the invention is evaluated by visually observing the inventive coating and comparing the HSCs of the invention to batch HSCs coated on PET films. HSC appearance can be reported, for example, according to the following rating system: HSCs with a "good" coating appearance as determined by visual observation versus HSCs with an "oily" coating appearance as determined by visual observation. HSCs with a "good" coating appearance are coatings where acceptable gloss and good smoothness of the coating are observed; and the "oily" coating appearance is that HSCs with ugly appearance are observed and are unacceptable. Additionally, by visual inspection, HSCs made using conventional batch processes can also appear undesirably "yellow" or opaque, whereas HSCs made according to the present invention do not have a "yellowing" appearance, but rather can be observed to have a clear coating.
For example, in one embodiment, the HSCs of the present invention have better sealing performance than batch processes in terms of adhesive strength. For example, the adhesive strength of the HSCs of the invention: from 20% to 300% better than the batch process in one embodiment, from 50% to 200% better than the batch process in another embodiment, and from 60% to 150% better than the batch process in yet another embodiment; and in yet another embodiment 70% to 100% better than the batch process. The sealing properties of HSCs were measured, for example, by the adhesion test as described in the examples below.
For example, in one embodiment, the hot-stick properties of the HSCs of the present invention are better than batch processes. For example, the hot tack properties of the HSCs of the invention: in one embodiment 10% to 200% better than the batch process, in another embodiment 20% to 150% better than the batch process, and in yet another embodiment 25% to 100% better than the batch process; and in yet another embodiment 30% to 80% better than the batch process. The thermal adhesive properties of HSCs are measured according to ASTM F1921 test method B, for example, using a temperature controlled Instron testing instrument (temperature controlled instrument) operating at a speed of 200 millimeters per second (mm/s).
As previously mentioned, the dispersion composition can be used to make HSCs for food packaging articles. Other applications in which the dispersion composition may be used include applications such as industrial skin packaging and medical packaging applications.
Examples of the invention
The following examples are presented to illustrate the invention in further detail, but should not be construed to limit the scope of the claims. All parts and percentages are by weight unless otherwise indicated.
Various terms and designations used in the following inventive examples (inv.ex.) and comparative examples (comp.ex.); and the raw materials or ingredients are described in table I.
TABLE I list of compounds
TABLE II compositional Properties
TABLE III Dispersion formula
TABLE IV-Dispersion conditions
Notes of Table IV:(1)“VaveragePS "stands for" volume average particle size ".
(2)"NA" stands for "not applicable".
(3)"ND" means "not dispersed".
(4)"NM" stands for "not measured".
Comparative examples A to D
General procedure for preparation of dispersions
The following general procedure was used to prepare aqueous dispersions in comparative examples a-D:
components 1-3 as described in Table IV were fed into a 25mm diameter twin screw extruder using a controlled rate feeder and using the feed rates (g/min) as described in Table IV. Components 1-3 are transferred through an extruder and melted to form a liquid molten material.
The extruder temperature profile was gradually raised to the temperature described in table IV under the column "polymer melt zone". Water and neutralizing agent were mixed together and fed into the extruder at the feed rate described in table IV to neutralize at the initial water introduction point. Next, two separate pumps were used to feed dilution water into the extruder at one inlet position or two separate inlet positions (first and second inlet positions) according to the feed rates described in table IV. The extruder temperature profile is cooled back to a temperature below 100 c near the end of the extruder. At the extruder outlet, a back pressure regulator was used to regulate the pressure inside the extruder barrel to a pressure suitable to reduce steam formation.
The aqueous dispersion product exits the extruder. The aqueous dispersion was filtered through a 200 μm filter. The resulting filtered aqueous dispersion has a solids content measured in weight percent (wt%); and the solid particles of the dispersion have a volume average particle size (V) measured in micronsAveragePS) and recorded in table IV. In some cases, the granularity modulus value is also recorded. Measuring the solids content of the aqueous dispersion using an infrared solids analyzer; and the particle size of the solid particles of the aqueous dispersion was measured using a coulter LS-230 particle size analyzer (available from beckmann coulter company). The solids content and the average Particle Size (PS) of the solid particles of the dispersion are described in table IV.
Examples 1 and 2 and comparative examples E-I
In inventive examples 1 and 2 and comparative examples E-I, aqueous dispersions were prepared using the general preparation procedure for dispersions described in comparative examples a-D above, but in which water and neutralizing agent were fed separately to the extruder after the extruder temperature profile was gradually raised to the temperature described in the column "polymer melt zone" of table IV. Water was fed into the extruder at the rate described in table IV, followed by addition of the neutralizing agent at the second introduction point at the rate described in table IV. After the neutralizing agent, the switching water is fed into the extruder at the inlet position of the extruder.
Measurement of properties
Measurement of solid content
The solids content of the dispersion was measured by an aohaus MB45 infrared moisture analyzer. The analyzer was set to 150 ℃, with measurement completion set to <1 milligram (mg) loss in 90 seconds(s).
Viscosity measurement
The viscosity of the dispersion was tested by Boehler fly DV-II +. Measurements were made using an RV rotor at 20 Revolutions Per Minute (RPM) and 25 ℃.
Particle size measurement
Particle size measurements of the dispersions were performed with a beckmann coulter LS 13320 instrument. The instrument was equipped with a universal liquid module containing DI water and the data was analyzed using an optical model with a fluid refractive index of 1.332 and a sample refractive index of 1.5 real and 0 imaginary parts.
Performance evaluation test
The performance of all dispersion compositions was evaluated by comparing the performance of the dispersions with the performance of commercial products made by the batch process. "batch Business" is available as Adcote 37JD1198 from Dow Chemical Company.
Coating the dispersion sample onto the substrate by hand using a meyer rod draw down bar and pull down method; and adjusting the dry coating weight to about 5.5-6.0g/m2. After the pull down, the wet coating was dried in an oven at 90 ℃ for about 2 minutes (min).
Storage stability
The storage stability of the dispersions under (1) refrigerated (4 ℃) ambient and (2) oven hot (45 ℃) aged conditions was evaluated by tracking phase separation and viscosity weekly. Comparing the overall stability of each dispersion to the batch process commercial product; and reporting the results according to the following rating system: dispersions having "good" shelf stability means dispersions that perform the same as commercial products in a batch process; and "worse" shelf stability means a dispersion that performs worse than a batch process commercial product.
Appearance of the coating
The appearance of HSCs formed from the dispersion on PET films was visually observed and compared to Adcote 37JD 1198. Coating appearance was reported according to the following rating system: HSCs with "good" coating appearance were observed to have coatings with acceptable gloss and good smoothness; whereas the "oily" coating appearance was observed to have an ugly oily appearance and was unacceptable.
Heat-sealable substrate
Preparing a heat-sealed substrate by heat-sealing the primed substrate to a second substrate using the following method:
the primed substrate comprised a commercially available 92g PET, pre-laminated PET-aluminum foil edge.
The second substrate comprised commercially available 92g PET, 4 mil polyvinyl chloride (PVC) sheeting, 4 mil polyethylene terephthalate glycol (PETG) sheeting, 4 mil Low Density Polyethylene (LDPE) sheeting, aluminum (Al) foil.
The dispersion composition of the present invention is applied to the surface of an undercoated substrate using a manual pull down procedure. The primed substrate coated with the wet dispersion composition is then contacted with a second substrate. The wet coated primed substrate and the second substrate were dried in a 90 ℃ oven for about 2 minutes. The dry target coat weight was adjusted to 5.5g/m2To 6.0g/m2。
Adhesion test of Heat-sealed substrates
Adhesion test of heat-sealed substrates was performed under the following conditions: at a pressure of 2.76 bar, over a period of 1.0 second, and at two different temperatures (93.33 ℃ and 121.11 ℃).
Using 25.4X 25.4mm2The sealed area of the tape was tested for adhesion at 254 mm/min. Three strips of each sample were tested and the average value reported.
Heat tack of heat-sealed substrates
Temperature control was used according to the method described in ASTM F1921 test method B
The test instrument (available from Instron) performs a heat tack measurement of the heat sealed substrate at a speed of 200 mm/s.
Shelf life stability
To evaluate shelf-life stability, samples were stored at 4 ℃ (in a refrigerator) and at 45 ℃ (in an oven) for different periods of time. The shelf-life stability of the samples was tested by visual observation and the test results are summarized in table V.
TABLE V storage stability of the dispersions
The shelf life stability in terms of viscosity of the dispersion after storage of the samples at 4 ℃ (in the refrigerator) and at 45 ℃ (in the oven) for various periods of time is summarized in table VI.
TABLE VI storage stability of the dispersions-viscosity
The samples of comparative example H and comparative example I produced a hazy oily coating appearance; no further adhesive strength tests were therefore performed on the samples of comparative example H and comparative example I.
Table VI-adhesion strength of coatings (90 ° peel test results-coated PET sealed to different substrates
TABLE VII-adhesive Strength of coatings (90 ℃ Peel test results-coated Tivick sealed to different substrates
(Tyvek)
TABLE VIII-adhesion strength of the coatings (90 ℃ peel test results)
Claims (16)
1. A method of making an aqueous dispersion composition using an extruder-based continuous process, the method comprising the steps of:
(A) providing an extruder;
(B) feeding into the extruder a mixture of: (i) at least one vinyl acetate copolymer; (ii) at least one compatibilizer; and a dispersant;
(C) feeding a first aqueous additive to the mixture of step (B) in the extruder to provide a continuous dispersion of polymer;
(D) feeding at least one base to the mixture of step (C) in the extruder to neutralize any effective acid present in the mixture of step (C); and
(E) feeding a second water addition to the mixture of step (D) in the extruder to effect a phase inversion to form an aqueous continuous dispersion.
2. The method of claim 1, wherein each of the components is: (i) at least one vinyl acetate copolymer; (ii) at least one compatibilizer; and (iii) at least one dispersing agent is separately fed into the extruder.
3. The method of claim 1, wherein the components are: (i) at least one vinyl acetate copolymer; (ii) at least one compatibilizer; and (iii) at least one dispersing agent is fed into the extruder together.
4. The method of claim 1, wherein the extruder has a first feed zone near a front end of the extruder, a second feed zone near a middle portion of the extruder, and a third feed zone near a back end of the extruder.
5. The process of claim 1, wherein the temperature of the first feeding zone is from 90 ℃ to 150 ℃.
6. The process of claim 1, wherein the temperature of the second feed zone is from 90 ℃ to 150 ℃.
7. The process of claim 1, wherein the temperature of the third feeding zone is from 80 ℃ to 150 ℃.
8. The process of claim 1, wherein the dispersion produced by the process has a shelf stability at room temperature of greater than 1 year and a particle size of less than 2 microns.
9. The method of claim 1, wherein the at least one vinyl acetate copolymer is an ethylene vinyl acetate copolymer and is fed into the extruder at a concentration of 50 to 90 weight percent of total solids.
10. The method of claim 1, wherein the at least one compatibilizer is a highly dimerized rosin acid and is fed into the extruder at a concentration of 5 to 30 weight percent of total solids.
11. The method of claim 1, wherein the at least one dispersant is oleic acid and is fed into the extruder at a concentration of 0.1% to 5% by weight of total solids.
12. The method of claim 1, wherein the amount of water in the first water addition fed into the extruder is from 3.5 to 6 wt% of the total solids and first water addition.
13. The process of claim 1, wherein the at least one base component (e) is potassium hydroxide and is fed into the extruder at a concentration of 80% to 120% neutralization of the theoretical acid number of the component.
14. The method of claim 1, wherein the amount of water in the second water addition fed into the extruder is greater than or equal to 3.5 wt% of the total solids, first and second water additions.
15. The method of claim 1 wherein the aqueous dispersion composition is free of wax.
16. A heat-seal coating for food packaging or for industrial packaging comprising the dispersion composition produced by the method of claim 1.
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| CN108137979A (en) * | 2015-10-07 | 2018-06-08 | 陶氏环球技术有限责任公司 | The method for preparing aqueous heat-sealing coating composition |
| CN111225959A (en) * | 2017-10-31 | 2020-06-02 | 陶氏环球技术有限责任公司 | Process for preparing aqueous heat-seal coating composition |
Also Published As
| Publication number | Publication date |
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| WO2020214257A1 (en) | 2020-10-22 |
| US20220351980A1 (en) | 2022-11-03 |
| TW202039645A (en) | 2020-11-01 |
| AR118567A1 (en) | 2021-10-20 |
| MX2021012763A (en) | 2022-01-19 |
| JP2022529693A (en) | 2022-06-23 |
| BR112021020892A2 (en) | 2021-12-21 |
| EP3956384A1 (en) | 2022-02-23 |
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